CN102874863B - Synthetic method for zinc oxide nano-particles - Google Patents
Synthetic method for zinc oxide nano-particles Download PDFInfo
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- CN102874863B CN102874863B CN201210409475.7A CN201210409475A CN102874863B CN 102874863 B CN102874863 B CN 102874863B CN 201210409475 A CN201210409475 A CN 201210409475A CN 102874863 B CN102874863 B CN 102874863B
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Abstract
The invention discloses a method for synthetizing nano zinc oxide particles by utilizing high-temperature self-propagating reaction. The method includes: mixing chemically pure Al, CuO, ZnO and ZrO2 powder with grain size of 200 meshes according to a certain proportion, filling the powder in a graphite crucible and laying a layer of pyrophoric powder on the surface of the powder, generating self-propagation high-temperature reaction by igniting the pyrophoric powder, obtaining product in a stainless steel collector disposed at a position 30-40cm above the crucible, placing the collected product into a tubular furnace for annealing at the temperature of 150 DEG C-250 DEG C for 10-30min and carrying out slow furnace cooling to obtain a final product. The synthetic method for zinc oxide nano-particles is simple in process, low in equipment requirement, high in yield, high in purity and full of industrial production value.
Description
Technical field
The invention belongs to the synthetic field of nano material, be specifically related to the self propagating high temperature synthetic method of a zinc oxide nanoparticles.
Background technology
In order to realize the restriction (especially UV-light) of some occasion to light radiation, the sensor that need to have the material of good uv absorption capacity or have outstanding photoelectric properties limits or surveys ultraviolet radiation.At field of Environment Protection, need the decomposition of the material promotion organic product with good catalyzed degradation effect.Meanwhile, the high speed development of hyundai electronics science and technology requires electronic component to less future development.There is the nano semiconductor material of outstanding ultraviolet light performance, catalyzed degradation performance, photoluminescence performance and photoelectric properties, caused the broad research of Chinese scholars, comprising zinc oxide.Zinc oxide relies on its good performance to become a kind of broad-spectrum material, in makeup, environmental protection and sensor manufacture, has important application.
The method of preparing at present Nano-class zinc oxide mainly concentrates on thermal evaporation chemical Vapor deposition process, thermal evaporation physical vaporous deposition, liquid phase direct reaction method, electrochemical deposition method, template, sol-gel method.Wherein physical vaporous deposition, chemical Vapor deposition process and template have higher requirement to equipment, are unfavorable for industrial production.And liquid phase direct reaction method, electrochemical deposition method, sol-gel method process are loaded down with trivial details, preparation time is long is also difficult to meet industrial requirement.
Summary of the invention
Technical problem to be solved by this invention is for the deficiencies in the prior art, the synthetic method of one zinc oxide nanoparticles is provided, and required equipment is simple, reaction is quick, and the nano granular of zinc oxide of preparing, there is very high purity, have suitable prospects for commercial application.
Zinc oxide nanoparticle synthetic method provided by the invention, the self propagating high temperature of Zinc oxide nanoparticle is synthetic, comprises the steps:
A) raw material is that granularity is 200 ~ 300 object Al, CuO, ZnO, ZrO
2powder, its massfraction is respectively Al 11.6% ~ 14.2%, CuO 24.4% ~ 28.3%, ZnO 28.2% ~ 32.3%, ZrO
229.3% ~ 31.7%, after fully being mixed, powder puts into plumbago crucible, then at powder surface paving one deck pyrophoric powders;
B) above plumbago crucible, 30 ~ 40 centimeters are placed the stainless steel collector of peviform; With the rifle of igniting, light powder, bring out self-propagating high-temperature reaction;
C) reaction obtains product after finishing in stainless steel collector, and product is the membranaceous stainless steel collector surface that covers;
D) product of collecting is placed in to tube furnace and anneals 10 ~ 30 minutes and furnace cooling at 150 ~ 250 degrees Celsius, obtain final product.
In such scheme, pyrophoric powders composition and mass ratio are 58%KNO
3, 18%Mg, 20%Al, 4%S.
The product of synthesized is that particle diameter is the spherical particle of zinc oxide of 250 nanometer left and right.
In this reaction system, aluminium powder and cupric oxide powder generation thermite reaction produce amount of heat, partial oxidation zinc is also with reactive aluminum generating portion heat and generate zinc, the zinc of generation and do not participate in the amount of heat liquefaction that the zinc oxide of reaction together produces by reaction and spray subsequently reaction vessels.In the air that is rich in oxygen, the zinc of ejection is collected by the stainless steel collector that oxidation is placed in 30 ~ 40 centimetres of reactor tops together with the zinc oxide drop of directly ejection rapidly, (150 ~ 250 degrees Celsius) furnace cooling after 10 ~ 30 minutes of annealing in tube furnace after collection, thus the uniform Nano-class zinc oxide particle of a large amount of particle diameters formed.Zirconium white is mainly used in regulating and controlling by the heat of absorption thermite reaction the severe degree of reaction.The reactional equation relating generally in reaction system is:
4Al+6CuO=2Al
2O
3+6Cu
2Al+3ZnO=Al
2O
3+3Zn
2Zn+O
2=2ZnO
Material characteristics prepared by the inventive method can be tested with following methods:
1 XRD test.After test, by the contrast peak of product and the characteristic peak of ZnO, can judge whether product is ZnO and whether contains other impurity.
2 sem tests.By the observation of scanning electron microscope, can obtain microscopic appearance and the microscopic dimensions of product.
The major advantage of present method has: matching requirements is low, simple to operate, reaction process is rapid, output is large, product purity is high.Product is the nano semiconductor material with outstanding ultraviolet light performance, catalyzed degradation performance, photoluminescence performance and photoelectric properties, need to shield UV-light and need to utilize the occasion of luminous energy decomposing organic pollutant to have a good application prospect.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, this invention is further illustrated.
Fig. 1 is the XRD diffract spectral line of the embodiment of the present invention 1 synthetic product, and in figure, each peak is the characteristic peak of zinc oxide, and the characteristic peak of other impurity does not observe, and proves that the purity of product is good.
Fig. 2 is the stereoscan photograph of the embodiment of the present invention 1 synthetic product, and in figure, product is spheroidal particle, by same scale contrast, can obtain particle diameter in 250 nanometer left and right.
Fig. 3 is the schematic diagram of the inventive method preparation facilities.
Embodiment
To contribute to understand by the following description of the embodiments the present invention, but not limit content of the present invention.
Embodiment 1
According to the mass ratio of 12.6:26.4:30.2:30.8, taking granularity is 200 object chemical pure Al, CuO, ZnO, ZrO
2powder, pours reaction vessel into after mixing, and at powder surface paving one deck pyrophoric powders, brings out self-propagating reaction with the rifle of the igniting pyrophoric powders that ignites.After reaction finishes, at the stainless steel collection device that is placed in more than reaction vessels 30 ~ 40 centimeters, obtain product, the product of collecting is placed in to tube furnace at 200 degrees Celsius of annealing 15 minutes furnace cooling.The finished product are through XRD analysis test and sem test.Test proves that product is high pure zinc oxide particle, and pattern is that spherical median size is in 250 nanometer left and right.
Embodiment 2
According to the mass ratio of 11.6:24.4:32.3:31.7, taking granularity is 200 object chemical pure Al, CuO, ZnO, ZrO
2powder, pours reaction vessel into after mixing, and at powder surface paving one deck pyrophoric powders, brings out self-propagating reaction with the rifle of the igniting pyrophoric powders that ignites.After reaction finishes, at the stainless steel collection device that is placed in more than reaction vessels 30 ~ 40 centimeters, obtain product, the product of collecting is placed in to tube furnace at 150 degrees Celsius of annealing ten minutes furnace cooling.The finished product are through XRD analysis test and sem test.Test proves that product is high pure zinc oxide particle, and pattern is that spherical median size is in 230 nanometer left and right.
Embodiment 3
According to the mass ratio of 14.2:28.3:28.2:29.3, taking granularity is 300 object chemical pure Al, CuO, ZnO, ZrO
2powder, pours reaction vessel into after mixing, and at powder surface paving one deck pyrophoric powders, brings out self-propagating reaction with the rifle of the igniting pyrophoric powders that ignites.After reaction finishes, at the stainless steel collection device that is placed in more than reaction vessels 30 ~ 40 centimeters, obtain product, the product of collecting is placed in to tube furnace at 250 degrees Celsius of annealing 30 minutes furnace cooling.The finished product are through XRD analysis test and sem test.Test proves that product is high pure zinc oxide particle, and pattern is that spherical median size is in 270 nanometer left and right.
Claims (2)
1. the synthetic method of a zinc oxide nanoparticles, is characterized in that, comprises the steps:
A) raw material is granularity 200～300 object Al, CuO, ZnO, ZrO
2powder, its massfraction is respectively Al 11.6% ~ 14.2%, CuO 24.4% ~ 28.3%, ZnO 28.2% ~ 32.3%, ZrO
229.3% ~ 31.7%, after powder is fully mixed, put into plumbago crucible, then at powder surface paving one deck pyrophoric powders, described pyrophoric powders composition and mass ratio are 58%KNO
3, 18%Mg, 20%Al, 4%S;
B) above plumbago crucible, 30 ~ 40 centimeters are placed the stainless steel collector of peviform; With the rifle of igniting, light pyrophoric powders, bring out self-propagating high-temperature reaction;
C) reaction obtains product after finishing in stainless steel collector, and product is the membranaceous stainless steel collector surface that covers;
D) product of collecting is placed in to tube furnace and anneals 10 ~ 30 minutes and furnace cooling at 150 ~ 250 degrees Celsius, obtain Zinc oxide nanoparticle.
2. synthetic method according to claim 1, is characterized in that, the Zinc oxide nanoparticle of synthesized is that particle diameter is the spherical particle of 250 nanometer left and right.
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| CN103318947B (en) * | 2013-07-08 | 2015-08-19 | 武汉大学 | A kind of burning synthesis method of ZnO nanoparticle |
| CN105755281B (en) * | 2016-04-01 | 2017-12-01 | 北京工业大学 | A kind of method based on self-propagating reaction processing zinc sulfide concentrates |
| CN107364885B (en) * | 2017-06-29 | 2019-05-31 | 武汉大学苏州研究院 | A method of utilizing the spherical bismuth oxide of Self-propagating Reaction Synthesis submicron order |
| CN107416907B (en) * | 2017-09-21 | 2019-02-12 | 华中农业大学 | A kind of preparation method of manganese oxide nanosphere |
| CN109455755B (en) * | 2018-09-25 | 2021-05-11 | 中国人民解放军陆军工程大学 | Zinc oxide nanowire and preparation method thereof |
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| CN1456495A (en) * | 2003-06-04 | 2003-11-19 | 北京科技大学 | Method for preparing aluminium nitrides and nitrogen oxides by combustion synthesis |
| CN102284263A (en) * | 2011-06-14 | 2011-12-21 | 武汉大学 | Method for synthesizing SnO2/SiO2 core-shell nanospheres |
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| US7897135B2 (en) * | 2004-09-27 | 2011-03-01 | University Of Houston | Carbon combustion synthesis of oxides |
| JP2008075105A (en) * | 2006-09-19 | 2008-04-03 | Naoyuki Kanetake | Composite material and its production method |
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| CN1456495A (en) * | 2003-06-04 | 2003-11-19 | 北京科技大学 | Method for preparing aluminium nitrides and nitrogen oxides by combustion synthesis |
| CN102284263A (en) * | 2011-06-14 | 2011-12-21 | 武汉大学 | Method for synthesizing SnO2/SiO2 core-shell nanospheres |
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